CN113831103A - Preparation method of high-temperature-resistant alumina-silica aerogel composite material - Google Patents
Preparation method of high-temperature-resistant alumina-silica aerogel composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000843 powder Substances 0.000 claims abstract description 49
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000835 fiber Substances 0.000 claims abstract description 33
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000010703 silicon Substances 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 239000003605 opacifier Substances 0.000 claims abstract description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005470 impregnation Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 239000004964 aerogel Substances 0.000 claims description 34
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 20
- 239000003054 catalyst Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 239000011240 wet gel Substances 0.000 claims description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 12
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000007598 dipping method Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000000748 compression moulding Methods 0.000 claims description 8
- 238000012216 screening Methods 0.000 claims description 8
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 7
- 229910052863 mullite Inorganic materials 0.000 claims description 7
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- 239000003365 glass fiber Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000000352 supercritical drying Methods 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 3
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 239000003377 acid catalyst Substances 0.000 claims description 2
- -1 alkyl alkoxy silane Chemical compound 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 2
- IWICDTXLJDCAMR-UHFFFAOYSA-N trihydroxy(propan-2-yloxy)silane Chemical compound CC(C)O[Si](O)(O)O IWICDTXLJDCAMR-UHFFFAOYSA-N 0.000 claims description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 239000011148 porous material Substances 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a preparation method of a high-temperature-resistant alumina-silica aerogel composite material, which comprises the following steps: (1) fully dispersing and mixing the nano alumina powder, the micron alumina powder, the infrared opacifier and the short fibers to obtain a mixture A; (2) pressing and forming the mixture A to obtain an alumina composite material; (3) uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol; (4) impregnating the alumina composite material by adopting silica sol; (5) drying to obtain the high-temperature resistant alumina-silica aerogel composite material. According to the invention, the compounding of the alumina and the silica aerogel is realized through impregnation, a complex preparation process is avoided, the preparation period is shortened, the silica aerogel is fixed in the alumina composite material, the compactness of the alumina composite material is further increased, the mechanical property is better, and the alumina composite material is prevented from generating large shrinkage at high temperature.
Description
Technical Field
The invention belongs to the field of heat insulation materials, and particularly relates to a preparation method of a high-temperature-resistant alumina-silica aerogel composite material.
Background
With the flying speed of the aircraft becoming faster and the surface temperature becoming higher and higher, the thermal insulation effect and the mechanical property of the conventional aluminum silicate or mullite fiber cannot meet the thermal protection requirement of the aerospace aircraft at a high temperature section, and the use of the novel nano aerogel thermal insulation composite material becomes the leading direction of high-efficiency thermal insulation.
Aerogel is the most ideal light heat-insulating material at present, is a light, amorphous and porous solid material composed of nano colloidal particles or high polymer molecules, and has extremely low density, high specific surface area and high porosity. The pore size of the aerogel (< 50nm) is smaller than the mean free path of air molecules (about 70 nm), there is no air convection inside the pores of the aerogel, and thus there is extremely low gaseous heat conduction; meanwhile, the aerogel has extremely high porosity and low volume ratio of solid, so that the solid heat conduction is very low, so that the aerogel has extremely low heat conductivity and is considered as the solid material with the best heat insulation performance found at present.
Currently, aerogel composite materials of silica system are widely researched and applied, but silica aerogel has no shielding capability to infrared rays with the wave band ranging from 2 μm to 8 μm. At high temperatures, the thermal radiation energy in this band will pass almost entirely through the aerogel. Meanwhile, at high temperature, the nano pores of the silicon dioxide aerogel easily collapse, the aerogel structure tends to be densified, and the temperature of the silicon dioxide aerogel cannot be higher than 650 ℃ when the silicon dioxide aerogel is used for a long time. Therefore, the availability of high temperature resistant aerogel thermal insulation composites that are resistant to infrared radiation would be of great significance to the development of high speed aircraft.
Among many aerogels, alumina aerogel has not only low thermal conductivity but also good high temperature (e.g., temperatures higher than 1050 ℃ in the case of long-term use) stability, and is an ideal material for preparing high temperature resistant heat insulating materials. However, alumina aerogel has a disadvantage that it undergoes crystal transition at high temperature to cause structural collapse and tends to shrink at high temperature. The method of mixing silica and alumina sol is a common method for improving the temperature resistance of silica aerogel at present. However, the low strength, brittleness, poor infrared radiation blocking capability, and difficulty in forming inherent in alumina-silica aerogel materials limit the industrial applicability of alumina-silica aerogels. Therefore, the preparation of the alumina-silica aerogel composite material with the use temperature of more than 1200 ℃ and better heat insulation performance and mechanical property has very important practical significance.
Disclosure of Invention
The invention aims to provide a preparation method of a high-temperature-resistant alumina-silica aerogel composite material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a high-temperature-resistant alumina-silica aerogel composite material is characterized by comprising the following steps:
(1) fully dispersing and mixing the nano-alumina powder, the micron-alumina powder, the infrared light-screening agent and the short fibers to obtain a mixture A, wherein the mass parts of the nano-alumina powder, the micron-alumina powder, the infrared light-screening agent and the short fibers are 45-65: 0-5: 35-50: 2-10;
(2) pressing and forming the mixture A in the step (1) to obtain an aluminum oxide composite material;
(3) preparing silica sol: uniformly mixing a silicon source, ethanol and water, adding a catalyst, and uniformly stirring to obtain a silicon dioxide sol;
(4) and (3) dipping treatment: dipping the alumina composite material obtained in the step (2) in the silica sol obtained in the step (3) to obtain an alumina-silica wet gel material;
(5) and (3) drying treatment: and (4) drying the alumina-silica wet gel material obtained in the step (4) to obtain the high-temperature-resistant alumina-silica aerogel composite material.
Preferably, in the step (1), the nano alumina powder is one or two of nano alumina aerogel powder and nano gas-phase alumina powder; the micron alumina powder is one or two of micron alumina aerogel powder and micron gas phase alumina powder; the infrared opacifier is one of nano silicon carbide, micron silicon carbide, nano titanium dioxide, micron titanium dioxide, nano zirconia and micron zirconia; the short fibers are 50-500 mu m in length and are one or more of carbon fibers, boron fibers, silicon carbide fibers, silicon nitride fibers, quartz fibers, alumina fibers, zirconia fibers, glass fibers, aluminum silicate fibers and mullite fibers.
Preferably, in the step (2), the pressure of the compression molding is 5-7.5MPa, and the dwell time is 40-100 s.
Preferably, in the step (3), the silica sol is obtained by mixing a silicon source, ethanol and water in a molar ratio of 1 to (2-60) to (1-30); the silicon source is one or more of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkylalkoxysilane includes one or more of methyltrimethoxysilane, dimethyldimethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, vinyltriethoxysilane, propyltrimethoxysilane, or propyltriethoxysilane.
Preferably, in the step (3), the catalyst is one or a combination of two of basic catalysts such as sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution, and the catalyst adjusts the pH of the silica sol to 6-8; also comprises adding an acid catalyst into the silica sol and adjusting the pH of the solution to 2-6.
Preferably, in the step (4), the impregnation is one of atmospheric pressure impregnation and pressurized impregnation.
Preferably, the step (5) of drying further comprises an aging process before the drying process, specifically, the alumina-silica wet gel material is aged for 8-24 hours at room temperature or under the condition of heating to 30-60 ℃.
Preferably, the drying treatment in step (5) is one of supercritical drying, freeze drying and atmospheric drying.
Preferably, the high-temperature resistant alumina-silica aerogel composite material prepared by the method.
Preferably, the thermal conductivity coefficient of the prepared alumina-silica aerogel composite material at normal temperature is as follows: 0.021-0.025 w/(m.cndot.), and has a thermal conductivity of 0.06-0.10 w/(m.cndot.) at 1000 ℃.
The invention has the beneficial effects that:
the alumina composite material in the high-temperature resistant alumina-silica aerogel composite material is prepared by pressing and molding nano alumina powder, micron alumina powder, an infrared opacifier and short fibers, the obtained alumina composite material has good mechanical property, a good framework structure is provided for the next preparation of the alumina-silica aerogel composite material, and on the other hand, the infrared opacifier is added in the pressing and molding process, so that the high-temperature infrared radiation heat conduction is well inhibited.
According to the invention, silica sol is impregnated in the prepared alumina composite material to obtain the alumina-silica aerogel composite material, and the alumina and silica aerogel are compounded by impregnation, so that a complex preparation process is avoided, and the preparation period is shortened; the silica aerogel is fixed in the alumina composite material, so that the compactness of the alumina composite material is further increased; the alumina powder is adopted for compression molding, so that the alumina composite material can be better prevented from generating larger shrinkage at high temperature, and the alumina-silica aerogel composite material with better heat insulation performance and mechanical property is prepared.
Detailed Description
In order that those skilled in the art will be able to better understand the technical solutions provided by the present invention, the following description is provided in connection with specific embodiments.
Example 1: a preparation method of a high-temperature-resistant alumina-silica aerogel composite material is characterized by comprising the following steps:
(1) fully dispersing and mixing the nano alumina aerogel powder, the micron silicon carbide infrared opacifier and the alumina short fibers to obtain a mixture A, wherein the mass parts of the nano alumina aerogel powder, the micron silicon carbide infrared opacifier and the alumina short fibers are = 60: 45: 8;
(2) performing compression molding on the mixture A in the step (1) under 7.5MPa, and maintaining the pressure for 40s to obtain an aluminum oxide composite material;
(3) preparing silica sol: uniformly mixing a silicon source, ethanol and water, adding a catalyst, and uniformly stirring to obtain a silicon dioxide sol;
(4) and (3) dipping treatment: pressurizing and dipping the alumina composite material obtained in the step (2) in the silica sol obtained in the step (3) to obtain an alumina-silica wet gel material;
(5) and (3) drying treatment: and (4) carrying out supercritical drying treatment on the alumina-silica wet gel material obtained in the step (4) to obtain the high-temperature-resistant alumina-silica aerogel composite material.
Wherein, in the step (3), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 40: 15; the silicon source is methyl trimethoxy silane; the catalyst is an ammonia solution, and the catalyst adjusts the pH of the silica sol to 6.
The high-temperature-resistant alumina-silica aerogel composite material prepared by the method.
The high temperature resistant alumina-silica aerogel composite material obtained in the embodiment has a thermal conductivity of 0.023 w/(m.DEG C.) at normal temperature and a thermal conductivity of 0.08 w/(m.DEG C.) at 1000 ℃.
Example 2:
a preparation method of a high-temperature-resistant alumina-silica aerogel composite material is characterized by comprising the following steps:
(1) fully dispersing and mixing nano gas-phase alumina powder, micron alumina aerogel powder, a micron zirconia infrared opacifier, short-cut glass fibers and short-cut mullite fibers to obtain a mixture A, wherein the nano gas-phase alumina powder, the micron alumina aerogel powder, the micron zirconia infrared opacifier, the short-cut glass fibers and the short-cut mullite fibers are = 55: 4: 40: 3: 2 in parts by mass;
(2) performing compression molding on the mixture A in the step (1) under 6MPa, and maintaining the pressure for 70s to obtain an aluminum oxide composite material;
(3) preparing silica sol: uniformly mixing a silicon source, ethanol and water, adding a catalyst, and uniformly stirring to obtain a silicon dioxide sol;
(4) and (3) dipping treatment: dipping the alumina composite material obtained in the step (2) in the silica sol obtained in the step (3) at normal pressure to obtain an alumina-silica wet gel material;
(5) and (3) drying treatment: and (4) drying the alumina-silica wet gel material obtained in the step (4) at normal pressure to obtain the high-temperature-resistant alumina-silica aerogel composite material.
Wherein, in the step (3), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 6: 2; the silicon source is tetraethoxysilane and methyl orthosilicate; the catalyst was an ammonium fluoride solution and the pH of the silica sol was adjusted to 7 by the catalyst.
The high temperature resistant alumina-silica aerogel composite material obtained in the embodiment has a thermal conductivity of 0.025 w/(m.DEG C) at room temperature and a thermal conductivity of 0.10 w/(m.DEG C) at 1000 ℃. .
Example 3:
a preparation method of a high-temperature-resistant alumina-silica aerogel composite material is characterized by comprising the following steps:
(1) fully dispersing and mixing the nano-alumina aerogel powder, the nano-fumed alumina powder, the nano-titanium dioxide infrared light-screening agent and the chopped carbon fibers to obtain a mixture A, wherein the mass parts of the nano-alumina aerogel powder, the nano-fumed alumina powder, the nano-titanium dioxide infrared light-screening agent and the chopped carbon fibers are = 20: 25: 35: 2;
(2) performing compression molding on the mixture A in the step (1) under 5MPa, and maintaining the pressure for 100s to obtain an aluminum oxide composite material;
(3) preparing silica sol: uniformly mixing a silicon source, ethanol and water, adding a catalyst, and uniformly stirring to obtain a silicon dioxide sol;
(4) and (3) dipping treatment: pressurizing and dipping the alumina composite material obtained in the step (2) in the silica sol obtained in the step (3) to obtain an alumina-silica wet gel material;
(5) aging: carrying out aging treatment on the alumina-silica wet gel material prepared in the step (4) for 24 hours at room temperature;
(6) and (3) drying treatment: and (4) carrying out supercritical drying treatment on the alumina-silica wet gel material obtained in the step (5) to obtain the high-temperature-resistant alumina-silica aerogel composite material.
Wherein, in the step (3), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 60: 30; the silicon source is dimethyl dimethoxy silane, methyl triethoxy silane and dimethyl diethoxy silane; the catalyst is ammonia water and ammonium fluoride aqueous solution, and the pH of the silica sol is adjusted to 8 by the catalyst.
The high temperature resistant alumina-silica aerogel composite material obtained in the embodiment has a thermal conductivity of 0.021 w/(m.DEG C) at normal temperature, and a thermal conductivity of 0.06 w/(m.DEG C) at 1000 ℃.
Example 4:
the present embodiment is the same as embodiment 3, and the description thereof is not repeated, except that:
(1) fully dispersing and mixing nano alumina aerogel powder, nano gas-phase alumina powder, micron alumina aerogel powder, nano silicon carbide infrared opacifier and short carbon fiber to obtain a mixture A, wherein the mass parts of the nano alumina aerogel powder, the nano gas-phase alumina powder, the micron alumina aerogel powder, the nano silicon carbide infrared opacifier and the short carbon fiber are 35: 30: 5: 50: 10;
the high temperature resistant alumina-silica aerogel composite material obtained in the embodiment has a thermal conductivity of 0.022 w/(m.DEG C) at normal temperature and a thermal conductivity of 0.07 w/(m.DEG C) at 1000 ℃.
Comparative example 1:
(1) fully dispersing and mixing nano gas-phase alumina powder, micron alumina aerogel powder, a micron zirconia infrared opacifier, short-cut glass fibers and short-cut mullite fibers to obtain a mixture A, wherein the nano gas-phase alumina powder, the micron alumina aerogel powder, the micron zirconia infrared opacifier, the short-cut glass fibers and the short-cut mullite fibers are = 55: 4: 40: 3: 2 in parts by mass;
(2) performing compression molding on the mixture A in the step (1) under 6MPa, and maintaining the pressure for 70s to obtain an aluminum oxide composite material;
the silica aerogel material obtained by the comparative example has a thermal conductivity of 0.026 w/(m.cndot.) at room temperature and a thermal conductivity of 0.12 w/(m.cndot.) at 1000 ℃.
Comparative example 2:
(1) fully dispersing and mixing nano alumina aerogel powder, nano silica aerogel powder, micron silicon carbide infrared light-screening agent and alumina short fibers to obtain a mixture A, wherein the mass parts of the nano alumina aerogel powder, the nano silica aerogel powder, the micron silicon carbide infrared light-screening agent and the alumina short fibers are 25: 40: 4;
(2) and (2) performing compression molding on the mixture A in the step (1) under 7.5MPa, and maintaining the pressure for 40s to obtain the alumina-silica aerogel composite material.
The alumina-silica aerogel composite material obtained by the comparative example has a thermal conductivity of 0.027 w/(m.DEG C) at room temperature and a thermal conductivity of 0.13 w/(m.DEG C) at 1000 ℃.
Claims (10)
1. A preparation method of a high-temperature-resistant alumina-silica aerogel composite material is characterized by comprising the following steps:
(1) fully dispersing and mixing the nano-alumina powder, the micron-alumina powder, the infrared light-screening agent and the short fibers to obtain a mixture A, wherein the mass parts of the nano-alumina powder, the micron-alumina powder, the infrared light-screening agent and the short fibers are 45-65: 0-5: 35-50: 2-10;
(2) pressing and forming the mixture A in the step (1) to obtain an aluminum oxide composite material;
(3) preparing silica sol: uniformly mixing a silicon source, ethanol and water, adding a catalyst, and uniformly stirring to obtain a silicon dioxide sol;
(4) and (3) dipping treatment: dipping the alumina composite material obtained in the step (2) in the silica sol obtained in the step (3) to obtain an alumina-silica wet gel material;
(5) and (3) drying treatment: and (4) drying the alumina-silica wet gel material obtained in the step (4) to obtain the high-temperature-resistant alumina-silica aerogel composite material.
2. The preparation method of the high-temperature-resistant alumina-silica aerogel composite material as claimed in claim 1, wherein in the step (1), the nano alumina powder is one or two of nano alumina aerogel powder and nano gas-phase alumina powder; the micron alumina powder is one or two of micron alumina aerogel powder and micron gas phase alumina powder; the infrared opacifier is one of nano silicon carbide, micron silicon carbide, nano titanium dioxide, micron titanium dioxide, nano zirconia and micron zirconia; the short fibers are 50-500 mu m in length and are one or more of carbon fibers, boron fibers, silicon carbide fibers, silicon nitride fibers, quartz fibers, alumina fibers, zirconia fibers, glass fibers, aluminum silicate fibers and mullite fibers.
3. The method for preparing a refractory alumina-silica aerogel composite according to claim 1, wherein in step (2), the pressure of the compression molding is 5-7.5MPa, and the dwell time is 40-100 s.
4. The preparation method of the high-temperature-resistant alumina-silica aerogel composite material as claimed in claim 1, wherein in the step (3), the silica sol is prepared by mixing a silicon source, ethanol, water = 1: (2-60): (1-30) in a molar ratio; the silicon source is one or more of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkylalkoxysilane includes one or more of methyltrimethoxysilane, dimethyldimethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, vinyltriethoxysilane, propyltrimethoxysilane, or propyltriethoxysilane.
5. The method according to claim 1, wherein in the step (3), the catalyst is one or a combination of two of basic catalysts such as sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution, and the catalyst adjusts the pH of the silica sol to 6-8; also comprises adding an acid catalyst into the silica sol and adjusting the pH of the solution to 2-6.
6. The method of claim 1, wherein in step (4), the impregnation is one of atmospheric pressure impregnation and pressure impregnation.
7. The preparation method of the high temperature resistant alumina-silica aerogel composite material according to claim 1, wherein the step (5) of drying further comprises an aging process, specifically, the alumina-silica wet gel material is aged for 8-24 hours at room temperature or at 30-60 ℃ after being heated.
8. The method of claim 1, wherein the drying process in step (5) is one of supercritical drying, freeze drying and atmospheric drying.
9. A refractory alumina-silica aerogel composite prepared by the method of any of claims 1 to 8.
10. The alumina-silica aerogel composite prepared by the method of any one of claims 1 to 8 has a thermal conductivity of 0.021 to 0.025 w/(m.cndot.) at ambient temperature and a thermal conductivity of 0.06 to 0.10 w/(m.cndot.) at 1000 ℃.
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